[go: up one dir, main page]

US4482658A - Process and apparatus for preparing aqueous dispersions of synthetic resins - Google Patents

Process and apparatus for preparing aqueous dispersions of synthetic resins Download PDF

Info

Publication number
US4482658A
US4482658A US06/449,986 US44998682A US4482658A US 4482658 A US4482658 A US 4482658A US 44998682 A US44998682 A US 44998682A US 4482658 A US4482658 A US 4482658A
Authority
US
United States
Prior art keywords
water
synthetic resin
milling means
solutions
milling
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
US06/449,986
Other languages
English (en)
Inventor
Friedrich Vock
Peter Lessmeister
Ralf Kirchner
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF Farben und Fasern AG
Original Assignee
BASF Farben und Fasern AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by BASF Farben und Fasern AG filed Critical BASF Farben und Fasern AG
Assigned to BASF FARBEM + FASERN AKTIENGESELLSCHAFT reassignment BASF FARBEM + FASERN AKTIENGESELLSCHAFT ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: KIRCHNER, RALF, LESSMEISTER, PETER, VOCK, FRIEDRICH
Application granted granted Critical
Publication of US4482658A publication Critical patent/US4482658A/en
Assigned to BASF LACKE + FARBEN AKTIENGESELLSCHAFT reassignment BASF LACKE + FARBEN AKTIENGESELLSCHAFT CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: BASF FARBEN + FASERN AKTIENGESELLSCHAFT
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/12Powdering or granulating
    • C08J3/14Powdering or granulating by precipitation from solutions
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/05Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from solid polymers

Definitions

  • the field of the invention is a process for preparing aqueous dispersions of synthetic resins and an apparatus for the production of these dispersions.
  • the invention is particularly concerned with the preparation of aqueous synthetic resin dispersions by precipitating the synthetic resins from their solutions in water miscible solvents with water.
  • the solutions may also contain pigments, fillers, and additives and the precipitation is simultaneously mechanically stressed by milling means, the precipitated solids are subsequently separated and uniformly distributed in an aqueous medium.
  • the particle size distribution of the solid ingredients affects greatly the property profile of many liquid system properties, for instance the stability of sedimentation, applicability, flow properties during film formation and the properties of the deposited and hardened films, for instance the color intensity and the gloss. Accordingly, specific distributions of particle sizes are required for specific products and applications, where these distributions should be below 10 microns for primer surfacers, motor vehicle primers and automobile top coats.
  • the particle sizes of synthetic resins in aqueous synthetic resin dispersions should also be of the same order of magnitude as the particle sizes of the pigments for these fields of application. This is not achieved however when synthetic resin solutions in organic solvents are atomized with gases, superheated steam, air or natural gas.
  • the atomized products then are dried and the solid, solvent-free synthetic resin particles so obtained are dispersed in water to form a synthetic resin dispersion.
  • the required particle sizes and a uniform distribution of grain sizes again are not achieved when a synthetic resin solution in organic solvents is distributed in water in an agitator, whereby the solid is precipitated. Again no good results are obtained when a synthetic resin solution in organic solvents is blown by means of jet nozzles into water, the solid being precipitated in this manner.
  • aqueous synthetic resin dispersions by precipitating the synthetic resins with water from their solutions in water miscible solvents, which may also contain pigments, fillers and additives, while simultaneously mechanically stressing the dispersions with milling means, whereupon the precipitated solids are separated and uniformly distributed in an aqueous medium.
  • the present invention is characterized in that the synthetic resins are precipitated in the presence of inert and moving milling means.
  • the synthetic resin solution is added with stirring to a vessel holding water and milling means, the precipitation of the solids taking place in particularly fine form due to the action of the milling means, the precipitate together with the liquid being separated from the milling means, the precipitate being filtered or centrifuged, and the filter cake or the centrifuged residue being dispersed into an aqueous medium.
  • Another embodiment of the invention provides continuous operation, using a continuously operating stirring mill.
  • the stirring mill includes circulating water introduced directly before the intake of the stirring mill or else parallel with this intake into the synthetic resin solution.
  • the precipitation takes place in the stirring mill within which remain the milling means while the precipitate together with the liquid is evacuated.
  • the advantages of the present invention using the milling means is that substantially finer particles of synthetic resins can be obtained and a very rapid precipitation procedure is possible.
  • the suitable milling means are inert and may consist of various materials. They are, for example, balls made of steel or glass, further of steatite, porcelain, flint, or also they are sand, such as Ottawa sand, for use in the stirring mills.
  • FIG. 1 is a schematic representation showing the present invention using a container filled with the milling means
  • FIG. 2 is a schematic representation showing the present invention using a stirring mill operating continuously.
  • FIG. 1 shows an agitation vessel (1) provided with a stirrer (2) and containing milling means (3).
  • Water (4) is present in the agitation vessel (1).
  • the stirrer (2) is rotated about its vertical axis, whereby the milling means (3) and the water (4) are set into intensive motion.
  • a synthetic resin solution (5) is supplied from above to the agitation vessel (1). Stirring proceeds for some time after the entire solution of the synthetic resin has been distributed through the vessel.
  • the liquid mixture is allowed to drain through a sieve (6) mounted at the bottom of the vessel (1) and retaining the milling means (3) within the vessel, the water containing the solvent being separated by a pump (7) and a filter (8) from the synthetic resin particles.
  • the filter cake so produced in the filter (8) can be washed with further water.
  • the water humid filter cake is dispersed in a container (9) using water and possibly dispersants and protective colloids to form a synthetic resin dispersion.
  • the mixture of water and solvent is fed through (10) to a solvent reprocessing apparatus.
  • water (4) is placed in an agitator vessel (1) provided with a stirrer (2), said water being pumped by a pump (11) through a stirring mill (12) filled with milling means and then being fed back into the vessel (1).
  • a solution of synthetic resin is metered at (13) into the above circulation.
  • the liquid mixture is supplied from the agitation vessel (1) through a three-way valve (14) to the filter or to the centrifuge (8).
  • the filter cake, or centrifuge residue, thereupon is dispersed with water into a synthetic resin dispersion.
  • aqueous dispersions prepared in this manner contain synthetic resin particles of minute size which are very finely distributed and which upon deposition on a substrate and hardening are indistinguishable in their technical properties from coatings made from a synthetic resin solution.
  • a solution is prepared from:
  • a flow agent such as MODAFLOW (R) in a ball mill to form a fine particulate dispersion (Hegmann granularity: 5 to 10 microns).
  • the precipitation was carried out according to the apparatus of FIG. 1 in a cooled agitated vessel holding 12 liters (of about 20 cm diameter) and provided with a paddle mixer rotating at 650 rpm.
  • the temperature was kept at 30° C. during the precipitation procedure.
  • the suspension so obtained was separated from the milling means using a sieve in front of the bottom valve of the agitation vessel. After the suspension was centrifuged, a centrifuged cake with a water content of 55% and a solvent content of less than 2% was obtained.
  • the grain size was determined by microscopic measurement and found to be about 5 microns.
  • processing viscosity was adjusted by adding about 15% of water, and a film was applied on a metal panel using a flow-cup gun and thereupon baked at 185° C. for 20 minutes, evincing good optical and weather-industrial properties.
  • Example 1 An enamel according to Example 1, for which the proportion of diacetone alcohol is replaced by acetone, is precipitated in an apparatus according to FIG. 1 using steatite as the milling means, the temperature being 20° C. and the other conditions the same as in Example 1.
  • the microscopically ascertained grain size was about 20 microns.
  • the spray viscosity is adjusted by adding about 20% water and the substance is applied by a flow-cup gun, whereupon it is baked (20 minutes at 185°C.), resulting in a film with good optical and weather-industrial properties.
  • An enamel with a Hegmann granular fineness of less than 5 microns was prepared in a stirring mill from:
  • an agitated mill contains glass milling means of 1.5 mm diameter filling the 4-liter capacity to 75% and is crossed by a circulation of water with a rate of 100 liter/h; the enamel is supplied at about 30 liter/h by a pump to the circulating water at the intake of this agitated vessel.
  • the quantitative ratios are so selected that after precipitation, the ratio of enamel to water is 1:5.
  • the suspension so obtained is centrifuged to a water content of about 50% and to less than 1% of organic solvent.
  • the spray viscosity is set by adding about 25% of water, and this substance is applied by a flow-cup gun; after baking at 15 minutes and 190° C., a film with good optical and weather-industrial properties is obtained.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Paints Or Removers (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
US06/449,986 1980-10-04 1982-12-15 Process and apparatus for preparing aqueous dispersions of synthetic resins Expired - Fee Related US4482658A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3037575 1980-10-04
DE3037575A DE3037575C2 (de) 1980-10-04 1980-10-04 Verfahren zum Herstellen von wäßrigen Kunstharzdispersionen

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
US06304008 Continuation 1981-09-21

Publications (1)

Publication Number Publication Date
US4482658A true US4482658A (en) 1984-11-13

Family

ID=6113617

Family Applications (1)

Application Number Title Priority Date Filing Date
US06/449,986 Expired - Fee Related US4482658A (en) 1980-10-04 1982-12-15 Process and apparatus for preparing aqueous dispersions of synthetic resins

Country Status (7)

Country Link
US (1) US4482658A (es)
EP (1) EP0049787B1 (es)
JP (1) JPS5794021A (es)
AT (2) ATE7706T1 (es)
BR (1) BR8106375A (es)
DE (2) DE3037575C2 (es)
ES (1) ES8207204A1 (es)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5856381A (en) * 1996-04-29 1999-01-05 Basf Aktiengesellschaft Compounding of polymer dispersions
US20040220318A1 (en) * 2003-04-29 2004-11-04 Lepkowski Thaddeus J. Method for creating microsphere polymers and particles

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2831840A (en) * 1953-07-03 1958-04-22 Shell Dev Process for treating polymer coagulates
US2854426A (en) * 1954-08-11 1958-09-30 Dasher Rubber & Chemical Compa Process of milling synthetic rubber latex coagulum containing water
US2977351A (en) * 1956-06-28 1961-03-28 Phillips Petroleum Co Process for recovery of polyolefin by precipitation in water
US3090774A (en) * 1963-05-21 scoggin
US3432483A (en) * 1965-02-18 1969-03-11 Nat Distillers Chem Corp Continuous process for preparing finely divided polymers
US3544540A (en) * 1968-11-12 1970-12-01 Phillips Petroleum Co Temperature control system
US3862103A (en) * 1971-10-27 1975-01-21 Goodyear Tire & Rubber Method of recovering polymer from its solution
US4202965A (en) * 1977-09-26 1980-05-13 Mitsubishi Gas Chemical Company, Inc. Method for isolating solid polyarylene ester from its organic solvent solution

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE787544A (fr) * 1971-08-14 1973-02-14 Basf Ag Procede de preparation de poudres de vernis pigmentees
GB1465601A (en) * 1973-03-31 1977-02-23 Basf Ag Production of resins
DE2419330B2 (de) * 1973-04-23 1975-02-20 Union Carbide Corp., New York, N.Y. (V.St.A.) Verfahren zur Herstellung von sprühbaren Uberzugspulvern feiner Teilchengröße
JPS5244053A (en) * 1975-10-03 1977-04-06 Mitsui Toatsu Chem Inc Method for processing waste water containing synthetic amino resin
US4206161A (en) * 1976-10-18 1980-06-03 Dai Nippon Toryo Co., Ltd. Method of producing resin powder
JPS54126335A (en) * 1978-03-24 1979-10-01 Kubota Ltd Harvester
JPS5653755A (en) * 1979-10-09 1981-05-13 Mitsubishi Metal Corp Pulverizing mixing machine

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3090774A (en) * 1963-05-21 scoggin
US2831840A (en) * 1953-07-03 1958-04-22 Shell Dev Process for treating polymer coagulates
US2854426A (en) * 1954-08-11 1958-09-30 Dasher Rubber & Chemical Compa Process of milling synthetic rubber latex coagulum containing water
US2977351A (en) * 1956-06-28 1961-03-28 Phillips Petroleum Co Process for recovery of polyolefin by precipitation in water
US3432483A (en) * 1965-02-18 1969-03-11 Nat Distillers Chem Corp Continuous process for preparing finely divided polymers
US3544540A (en) * 1968-11-12 1970-12-01 Phillips Petroleum Co Temperature control system
US3862103A (en) * 1971-10-27 1975-01-21 Goodyear Tire & Rubber Method of recovering polymer from its solution
US4202965A (en) * 1977-09-26 1980-05-13 Mitsubishi Gas Chemical Company, Inc. Method for isolating solid polyarylene ester from its organic solvent solution

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5856381A (en) * 1996-04-29 1999-01-05 Basf Aktiengesellschaft Compounding of polymer dispersions
US20040220318A1 (en) * 2003-04-29 2004-11-04 Lepkowski Thaddeus J. Method for creating microsphere polymers and particles
US7022747B2 (en) * 2003-04-29 2006-04-04 Basf Corporation Method for creating microsphere polymers and particles

Also Published As

Publication number Publication date
DE3163903D1 (en) 1984-07-05
EP0049787A1 (de) 1982-04-21
EP0049787B1 (de) 1984-05-30
DE3037575A1 (de) 1982-04-22
ATA423581A (de) 1985-03-15
ES505998A0 (es) 1982-09-01
ATE7706T1 (de) 1984-06-15
BR8106375A (pt) 1982-06-22
ES8207204A1 (es) 1982-09-01
DE3037575C2 (de) 1982-12-02
JPS5794021A (en) 1982-06-11

Similar Documents

Publication Publication Date Title
US3561003A (en) Spray drying process
US2581414A (en) Process for dispersing pigments in film-forming materials
US3674736A (en) Process for the preparation of pigmented polymer powders of controlled particle shape and size and size distribution and product
AU643191B2 (en) Coloured powder coating compositions
US5854311A (en) Process and apparatus for the preparation of fine powders
EP0372860B1 (en) Coloured powder coating compositions
JPH08231890A (ja) 光沢のあるエマルジョンペイント
US4332354A (en) Process for preparing transparent iron oxide pigment dispersions
US4936913A (en) Aluminum flake pigment
CZ389992A3 (en) Process for preparing pulverized materials for the formation of heat-hardenable coatings and material for the formation of such coatings
US5824144A (en) Powder coating composition and method
FI59608B (fi) Foerfarande foer framstaellning av ett pulverformigt belaeggningsmaterial
EP0459048A1 (en) Coloured powder coating compositions
US4226634A (en) Process for preparing pigment compositions
US4482658A (en) Process and apparatus for preparing aqueous dispersions of synthetic resins
US5981696A (en) Process for preparing coating powder compositions and their use for making coatings
JPH11343432A (ja) 水性分散塗料の製造方法及び粉体塗料の製造方法
US4042560A (en) Method of preparing homogeneous thermosetting powder paint compositions
JPS60118754A (ja) 顔料分散方法
US6677484B1 (en) Melt-sprayed curing agent powder and powder coating compositions made therefrom
US4028326A (en) Process for producing powder paint particles from liquid paint I
US4028327A (en) Process for producing powder paint particles from liquid paint II
CA1053086A (en) Method of preparing powder particles by control of the particle shape
US6241382B1 (en) Method for producing powder lacquer containing gloss pigments
US2722485A (en) Method for producing coloring pigment

Legal Events

Date Code Title Description
AS Assignment

Owner name: BASF FARBEM + FASERN AKTIENGESELLSCHAFT AM NEUMARK

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNORS:VOCK, FRIEDRICH;LESSMEISTER, PETER;KIRCHNER, RALF;REEL/FRAME:004288/0014

Effective date: 19840718

Owner name: BASF FARBEM + FASERN AKTIENGESELLSCHAFT,GERMANY

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:VOCK, FRIEDRICH;LESSMEISTER, PETER;KIRCHNER, RALF;REEL/FRAME:004288/0014

Effective date: 19840718

FEPP Fee payment procedure

Free format text: PAYOR NUMBER ASSIGNED (ORIGINAL EVENT CODE: ASPN); ENTITY STATUS OF PATENT OWNER: LARGE ENTITY

AS Assignment

Owner name: BASF LACKE + FARBEN AKTIENGESELLSCHAFT

Free format text: CHANGE OF NAME;ASSIGNOR:BASF FARBEN + FASERN AKTIENGESELLSCHAFT;REEL/FRAME:004595/0752

Effective date: 19860811

FPAY Fee payment

Year of fee payment: 4

FEPP Fee payment procedure

Free format text: PAYER NUMBER DE-ASSIGNED (ORIGINAL EVENT CODE: RMPN); ENTITY STATUS OF PATENT OWNER: LARGE ENTITY

Free format text: PAYOR NUMBER ASSIGNED (ORIGINAL EVENT CODE: ASPN); ENTITY STATUS OF PATENT OWNER: LARGE ENTITY

FPAY Fee payment

Year of fee payment: 8

REMI Maintenance fee reminder mailed
LAPS Lapse for failure to pay maintenance fees
FP Lapsed due to failure to pay maintenance fee

Effective date: 19961113

STCH Information on status: patent discontinuation

Free format text: PATENT EXPIRED DUE TO NONPAYMENT OF MAINTENANCE FEES UNDER 37 CFR 1.362